반응 #72514

ord-8de85d599504467eb920c5fc0f296886

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출extracted with dichloromethane (3×70 mL)
  2. 2
    세척The combined organic extracts were washed with saturated aqueous sodium bicarbonate (100 mL)
  3. 3
    건조dried over anhydrous sodium sulfate
  4. 4
    여과filtered
  5. 5
    농축concentrated under reduced pressure

실험 절차

A solution of 5-methyl-2-nitrobenzoyl chloride (3.77 g, 18.9 mmol) in tetrahydrofuran (25 mL) was treated with a solution consisting of 2-chloropyridin-3-amine (2.6 g, 20.22 mmol), pyridine (6 mL) and tetrahydrofuran (15 mL). The reaction mixture was stirred for 2 hours then diluted with water (150 mL) and extracted with dichloromethane (3×70 mL). The combined organic extracts were washed with saturated aqueous sodium bicarbonate (100 mL) and dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to afford N-(2-chloropyridin-3-yl)-5-methyl-2-nitrobenzamide (5.44 g) that was used without further purification. LCMS [M+H]: 292.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541407B2uspto-grants-2013_09